CN102560292B - Tungsten-based plasma facing material and preparation method thereof - Google Patents
Tungsten-based plasma facing material and preparation method thereof Download PDFInfo
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- CN102560292B CN102560292B CN2012100483239A CN201210048323A CN102560292B CN 102560292 B CN102560292 B CN 102560292B CN 2012100483239 A CN2012100483239 A CN 2012100483239A CN 201210048323 A CN201210048323 A CN 201210048323A CN 102560292 B CN102560292 B CN 102560292B
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Abstract
The invention discloses a tungsten-based plasma facing material and a preparation method thereof. The preparation method comprises the following steps: uniformly mixing tungsten powder and tungsten fiber by a powder mixing method which does not damage the tungsten fiber; and sintering to prepare a bulk fiber toughened tungsten-based material by a hot isostatic pressing process. The tungsten powder is one of pure tungsten powder, tungsten-rhenium alloy powder, and tungsten powder doped with carbide and oxide; and the tungsten fiber is a pure tungsten wire, a tungsten-rhenium alloy wire or the like. The tungsten-based plasma facing material has the advantages of high thermal conductivity, high melting point temperature, low sputtering yield, low hydrogen isotope retention and low vapor pressure, as well as low cost and greater toughness.
Description
Technical field
The present invention relates to fusion reactor flux of plasma material, is exactly a kind of tungsten based plasma facing material and preparation method thereof.
Background technology
The tungsten material is considered to prepare the important candidate material of the flux of plasma parts (plasma-facing components, PFC) of international thermonuclear fusion experimental reactor ITER and following Commercial Demonstration heap DEMO due to good characteristics such as its high-melting-point, high sputter threshold value, high heat conductance, low-vapor pressure, low hydrogen isotope delays.But the fragility of tungsten is to limit it is applied in fusion reactor PFC a important factor.It is generally acknowledged that its fragility source mainly contains three aspects: 1, a large amount of dislocation motions in tungsten often need high temperature to activate, research shows, the plasticity of tungsten material is mainly by 1/2<111 > motion control of helical dislocation, but the Peierls power of this dislocation motion large (being about 2.8GPa under room temperature); 2, often very difficult elimination of low solubility impurity in tungsten in Industrial processes, the detrimental impurity elements such as O, N, H weaken at the tungsten Grain Boundary Segregation fragility (this problem can be alleviated with the dilution impurity concentration by the working depth that increases tungsten) that crystal boundary often causes tungsten; 3, in fusion reactor, the residing high hot-fluid loading of PFC and high-energy neutron radiation environment often make tungsten be easy to occur recrystallize embrittlement and radiation embrittlement.Can assert, the fragility of tungsten can reduce the service life of PFC and then threaten fusion facility safety.So the toughness that improves the tungsten sill is one of important topic of fusionable material circle research.
At present for tungsten toughness reinforcing, carry out more research both at home and abroad, mainly comprised the alloy malleableize of rhenium element solid solution, " top-down " and the methods such as " bottom-up " of high-energy ball milling fragmentation powder and then HIP sintering of severe plastic deformation (being typically high pressure torsion and Equal-channel Angular Pressing) crystal grain thinning.But it seems that at present although the work of this respect has obtained very large effect, premature with regard to the engineering application.This just prepares and meets the tungsten sill that fusion requires in the urgent need to attempting new toughness reinforcing approach.
The fiber reinforced matrix material of ceramic base has obtained researching and developing widely and having obtained some industrial application in the recent decade.Its basic toughening mechanism can be understood as the cracking waste of energy at fiber/matrix interface and ensuing fiber in interface Frictional Slipping waste of energy.The foreign scholar adds the analysis of the Push-out experiment of sample of tungsten fiber and three-point bending test result to show waste of energy in the tungsten fiber moving process and the deflection of crackle for CVD tungsten, so has determined fiber reinforced concept is applied in the tungsten sill feasibility.
The standby toughness reinforcing tungsten base of the macrofiber PFM of chemical vapour deposition (CVD) legal system that abroad begun one's study at present, but this complex technical process, production efficiency is low and long stapled anisotropy, maybe will limit its development and application.For the toughness reinforcing tungsten base of the tungsten fiber of preparing block (tungsten fiber-toughened tungsten matrix composite, W that can fast and low-cost
f/ W) PFM, this patent has proposed a preparation method based on prior powder metallurgy technique.
Summary of the invention
The objective of the invention is for Existing Defects, provide a kind of except having the traditional advantage of tungsten material and can significantly improving fracture toughness property, have tungsten based plasma facing material of excellent over-all properties and preparation method thereof.
Above-mentioned purpose realizes by following scheme:
A kind of tungsten based plasma facing material is characterized in that: be to take tungsten powder and tungsten fiber to make as raw material, the proportioning that accounts for the about 10%-30% of matrix tungsten powder volume ratio by tungsten fiber is chosen tungsten powder; It is by the powder mixing method that utilization is unlikely to damage tungsten fiber, the tungsten powder powder to be mixed with tungsten fiber, then utilize the heat and other static pressuring processes sintering to prepare the fiber reinforced tungsten sill of block and obtain, and described tungsten powder is pure tungsten powder, W-Re alloys powder, a kind of in the tungsten powder powder of doping carbon compound or oxide compound, described tungsten fiber is the alloy fibers such as pure tungsten fiber or W-Re.
Described a kind of tungsten based plasma facing material is characterized in that: described pure tungsten powder size is 0.1-20 μ m, purity>99.5wt%, and the alloy in described W-Re alloys powder or alloy fiber refers to the tungstenalloy that contains the 0.5-10wt% rhenium; Content<the 5wt% of carbide or oxide compound in the tungsten powder of described doping carbon compound or oxide compound, adopt the nanophase doping; Described tungsten fiber is chopped strand, and its length is 1-5mm, and it is excessively curling that fiber should be avoided as far as possible.
Described a kind of tungsten based plasma facing material, it is characterized in that: the recrystallization temperature of described tungsten fiber need reach 2000K, and diameter is in 10-300 μ m left and right, and tensile strength need be more than 2.5GPa; Described tungsten powder impurities content need be low as far as possible, requires its purity>99% and grain-size<3 μ m.
The preparation method of described tungsten based plasma facing material is characterized in that: comprise the following steps:
A, take raw material by weight ratio, described tungsten fiber surface can not processed, perhaps in its surface coverage film or coating, with the powder mixing method that is unlikely to damage tungsten fiber, raw material is mixed again, in order to remove the gaseous impurities of powder absorption, batch mixing is placed in the gained powder to be better than 10 after finishing
-3In the vacuum of the Pa order of magnitude, be incubated 0.5-1 hour under 500-800 ℃;
B, the powder that steps A is mixed utilize the hot isostatic pressing method to carry out sintering, sintering time is 2-3 hour, pressure is 150-200MPa, working gas is argon gas, the sintering temperature of hot isostatic pressing can not surpass the origin of fibers recrystallization temperature, is advisable in the 1700K left and right, obtains the fiber reinforced tungsten sill of block, make again the parts of different shapes and size, obtain product.
The preparation method of described a kind of tungsten based plasma facing material; it is characterized in that: described be unlikely to damage tungsten fiber powder mixing method refer to the chopped one-tenth of the tungsten filament 1-5mm of diameter 10-300 μ m long; then by proportioning, choose tungsten powder and mix in the low energy ball mill; in order to prevent the contaminating impurity in mechanical milling process, mechanical milling process need carry out in the high-purity hydrogen protective atmosphere.
The preparation method of described a kind of tungsten based plasma facing material, it is characterized in that: described film or coating in the method for physical vaporous deposition or chemical Vapor deposition process or sol-gel method a kind of the preparation and obtain the about 100-300nm of coat-thickness.
The preparation method of described a kind of tungsten based plasma facing material is characterized in that: described film or coating are ZrO
2, La
2O
3, Y
2O
3, a kind of film or coating in C.
Beneficial effect of the present invention is:
1, the present invention combines powder metallurgical technique and fiber reinforced concept to apply to prepare W
f/ W-PFM, the low energy 3D mixed powder of mixed powder tank or other low energy powder mixing method that utilization is unlikely to damage tungsten fiber make powder and chopped tungsten fiber mix and remove adsorbed gas and then employing heat and other static pressuring processes, and making fast and low-cost prepare high tenacity tungsten base PFM becomes possibility; In tungsten-based composite material prepared by the present invention Fiber Distribution evenly and matrix present the equiax crystal shape, therefore mechanics and thermal conduction present isotropy.Under ITER rank pure tungsten room temperature, thermal conductivity is about 160W/mK, because the heat conduction of metallic substance is mainly undertaken by the motion of internal freedom electronics, the interface of tungsten material middle-high density (as tungsten grain size<2 μ m time crystal boundary) scattered electrons ability is very strong, can cause the reduction of thermal conductivity.The W related in the present invention
fThe compound principal character of/W is the interpolation of tungsten fiber and does not highlight grain refining, therefore can keep thermal conductivity preferably.Tungsten base PFM prepared by this technique can not sacrifice commercial tungsten material and as some advantages of PFM, exchange the toughness of tungsten material for, namely has advantages of conventional commercial tungsten sill, as high heat conduction, high-melting-point, low sputtering yield, low hydrogen isotope delay and low-vapor pressure etc.
2, the foreign scholar adopts chemical vapour deposition (CVD) method to prepare high-quality W
f/ W-PFC, needed condition is high purity WF
6(>99.9wt%), the temperature field of 550 ℃ of left and right and corresponding vacuum apparatus and tail gas (HF) treatment facility, prepare thicker sample and often need tens of hours.Therefore say for preparing block materials, cost is far away higher than the very ripe powder metallurgic method of technology.The starting material that the present invention relates to and production technique have industrial foundation widely, can utilize industrial chopped tungsten filament and high-quality reduction tungsten powder preparation, with low cost.
3, the tungsten fiber structure refinement degree of the present invention's employing is high, have high intensity, good plasticity, high recrystallization temperature and the strong anti-radiation performance of prolonging, fiber reinforced effect after matrix perfect recrystallization or more radiation defect still exist while existing, can extend the service life of PFC under the strong irradiation field operating mode of fusion reactor.Cracking waste of energy and ensuing fiber based on the fiber/matrix interface greatly improve the brittle behaviour of tungsten at the toughening effect of interface Frictional Slipping waste of energy.
Embodiment
Embodiment 1:
A kind of tungsten based plasma facing material is characterized in that: be to take tungsten powder and tungsten fiber to make as raw material, the proportioning that accounts for the about 10%-30% of matrix tungsten powder volume ratio by tungsten fiber is chosen tungsten powder; It is the tungsten powder powder to be mixed and the vacuum high-temperature degasification with tungsten fiber by the powder mixing method that utilization is unlikely to damage tungsten fiber, then utilize the heat and other static pressuring processes sintering to prepare the fiber reinforced tungsten sill of block and obtain, and described tungsten powder is pure tungsten powder, W-Re alloys powder, a kind of in the tungsten powder powder of doping carbon compound or oxide compound, described tungsten fiber is the alloy fibers such as pure tungsten fiber or W-Re.
Described a kind of tungsten based plasma facing material is characterized in that: described pure tungsten powder size is 0.1-20 μ m, purity>99.5wt%, and the alloy in described W-Re alloys powder or alloy fiber refers to the tungstenalloy that contains the 0.5-10wt% rhenium; Content<the 5wt% of carbide or oxide compound in the tungsten powder of described doping carbon compound or oxide compound, adopt the nanophase doping; Described tungsten fiber is chopped strand, and its length is 1-5mm, and it is excessively curling that fiber should be avoided as far as possible.
Described a kind of tungsten based plasma facing material, it is characterized in that: the recrystallization temperature of described tungsten fiber need reach 2000K, and diameter is in 10-300 μ m left and right, and tensile strength need be more than 2.5GPa; Described tungsten powder impurities content need be low as far as possible, requires its purity>99% and grain-size<3 μ m.
The preparation method of described tungsten based plasma facing material is characterized in that: comprise the following steps:
A, take raw material by weight ratio, described tungsten fiber surface can not processed, perhaps in its surface coverage film or coating, with the powder mixing method that is unlikely to damage tungsten fiber, raw material is mixed again, in order to remove the gaseous impurities of powder absorption, batch mixing is placed in the gained powder to be better than 10 after finishing
-3In the vacuum of the Pa order of magnitude, be incubated 0.5-1 hour under 500-800 ℃;
B, the powder that steps A is mixed utilize the hot isostatic pressing method to carry out sintering, sintering time is 2-3 hour, pressure is 150-200MPa, working gas is argon gas, the sintering temperature of hot isostatic pressing can not surpass the origin of fibers recrystallization temperature, is advisable in the 1700K left and right, obtains the fiber reinforced tungsten sill of block, make again the parts of different shapes and size, obtain product.
The preparation method of described a kind of tungsten based plasma facing material; it is characterized in that: described be unlikely to damage tungsten fiber powder mixing method refer to the chopped one-tenth of the tungsten filament 1-5mm of diameter 10-300 μ m long; then by proportioning, choose tungsten powder and mix in the low energy ball mill; in order to prevent the contaminating impurity in mechanical milling process, mechanical milling process need carry out in the high-purity hydrogen protective atmosphere.
The preparation method of described a kind of tungsten based plasma facing material, it is characterized in that: described film or coating in the method for physical vaporous deposition or chemical Vapor deposition process or sol-gel method a kind of the preparation and obtain the about 100-300nm of coat-thickness.
The preparation method of described a kind of tungsten based plasma facing material is characterized in that: described film or coating are ZrO
2, La
2O
3, Y
2O
3, a kind of film or coating in C.
The product made has advantages of conventional commercial tungsten sill, under ITER rank pure tungsten room temperature, thermal conductivity is greater than 160W/m*K, fusing point is greater than 3410 ℃, have advantages of that high heat conduction, high-melting-point degree centigrade, low sputtering yield, low hydrogen isotope are detained and low-vapor pressure, cost is low simultaneously, has larger toughness.Conventional commercial tungsten material can't be in draw stage generation viscous deformation, and this product has viscous deformation to a certain degree, illustrates that this product has certain toughness.
Embodiment 2:
1, buy high-quality business doped tungsten wire and reduction tungsten powder, require: the recrystallization temperature of doped tungsten wire need reach 2000K, and diameter is in 10-300 μ m left and right, and tensile strength need be more than 2.5GPa; Reduction tungsten powder impurities content need be low as far as possible, and (purity>99.5wt%) and grain-size as far as possible little (<3 μ m) are to improve the sintering quality;
2,, in order to improve the interface performance of tungsten fiber and tungsten basal body, need on tungsten filament, utilize the methods such as physics (chemistry) vapour deposition or sol-gel to prepare intermediate layer film, as ZrO
2, La
2O
3, Y
2O
3, the films/coatings such as C;
3, the chopped one-tenth of the tungsten filament 1-5mm of diameter 10-300 μ m is long, the proportioning that then accounts for the about 10%-30% of matrix volume ratio by fiber is chosen tungsten powder and mixes in the low energy ball mill, and batch mixing is placed in the gained powder to be better than 10 after finishing
-3Insulation 0.5-1h degasification under 500-800 ℃ in the vacuum of the Pa order of magnitude.
The powder that 4, will mix utilizes the hot isostatic pressing method to carry out sintering, and sintering temperature should be advisable in the 1700K left and right, and pressure is the 200MPa left and right, and working gas is argon gas, and jacket is selected the titanium material.
5, according to the design requirements of fusion reactor PFC, can be made by the heat and other static pressuring processes direct sintering parts of different shapes and size, or W prepared by sintering
f/ W materials processing becomes to require parts.
6, the product made has well kept commercial tungsten high-melting-point, high thermal conductance, the advantages such as low hydrogen isotope delay; The performance isotropy is better than tungsten continuous fiber matrix material prepared by CVD simultaneously; Because adopting the good starting material of industrial foundation and powder sintering, with low cost; The three-point bending test shows that this material can demonstrate the inelastic deformation ability that commercial polycrystalline tungsten does not possess, this is because in loading procedure, occurred that crackle, along fiber and basal body interface expansion and the further dissipation energy of the relative Frictional Slipping of debonding interface, has improved the toughness of fragility tungsten sill greatly.In sum, the Wf/W matrix material for preparing of the present invention is a kind of flux of plasma material had a extensive future.
Claims (3)
1. tungsten based plasma facing material is characterized in that: be to take tungsten powder and tungsten fiber to make as raw material, the proportioning that accounts for matrix tungsten powder volume ratio 10%-30% by tungsten fiber is chosen tungsten powder; It is by the powder mixing method that utilization is unlikely to damage tungsten fiber, the tungsten powder powder to be mixed with tungsten fiber, then utilize the heat and other static pressuring processes sintering to prepare the fiber reinforced tungsten sill of block and obtain, and described tungsten powder is pure tungsten powder, W-Re alloys powder, a kind of in the tungsten powder powder of doping carbon compound or oxide compound, described tungsten fiber is pure tungsten fiber or W-Re alloys fiber;
The preparation method of described tungsten based plasma facing material comprises the following steps:
A, take raw material by weight ratio, does not process on described tungsten fiber surface, perhaps in its surface coverage film or coating, with the powder mixing method that is unlikely to damage tungsten fiber, raw material is mixed again, in order to remove the gaseous impurities of powder absorption, batch mixing is placed in the gained powder to be better than 10 after finishing
-3In the vacuum of the Pa order of magnitude, be incubated 0.5-1 hour under 500-800 ℃;
B, the powder that steps A is mixed utilize the hot isostatic pressing method to carry out sintering, sintering time is 2-3 hour, pressure is 150-200MPa, working gas is argon gas, the sintering temperature of hot isostatic pressing can not surpass the origin of fibers recrystallization temperature, at 1700K, obtains the fiber reinforced tungsten sill of block, make again the parts of different shapes and size, obtain product;
Described be unlikely to damage tungsten fiber powder mixing method refer to the chopped one-tenth of the tungsten filament 1-5mm of diameter 10-300 μ m long, then by proportioning, choose tungsten powder and mix in the low energy ball mill, in order to prevent the contaminating impurity in mechanical milling process, mechanical milling process need carry out in the high-purity hydrogen protective atmosphere; Described film or coating in the method for physical vaporous deposition or chemical Vapor deposition process or sol-gel method a kind of the preparation and obtain coat-thickness 100-300 nm; Described film or coating are ZrO
2, La
2O
3, Y
2O
3, a kind of film or coating in C.
2. a kind of tungsten based plasma facing material according to claim 1, it is characterized in that: described pure tungsten powder size is 0.1-20 μ m, purity > 99.5wt%, the alloy in described W-Re alloys powder or alloy fiber refers to the tungstenalloy that contains the 0.5-10wt% rhenium; Content<the 5wt% of carbide or oxide compound in the tungsten powder of described doping carbon compound or oxide compound, adopt the nanophase doping; Described tungsten fiber is chopped strand, and its length is 1-5mm, and it is excessively curling that fiber should be avoided as far as possible.
3. a kind of tungsten based plasma facing material according to claim 1, it is characterized in that: the recrystallization temperature of described tungsten fiber need reach 2000K, and diameter is at 10-300 μ m, and tensile strength need be more than 2.5GPa; Described tungsten powder impurities content need be low as far as possible, requires its purity > 99% and grain-size<3 μ m.
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| CN110343978A (en) * | 2019-07-08 | 2019-10-18 | 西安理工大学 | The short tungsten fiber Reinforced Cu W composite material and preparation method of random distribution |
| CN110684936B (en) * | 2019-11-14 | 2021-02-05 | 北京科技大学天津学院 | Short-cut tungsten fiber reinforced vanadium-chromium-based composite material and preparation method thereof |
| CN112442643B (en) * | 2020-10-23 | 2021-08-27 | 合肥工业大学 | Layered fiber toughened tungsten-based composite material and preparation method thereof |
| CN113488202A (en) * | 2021-06-18 | 2021-10-08 | 中国科学院合肥物质科学研究院 | Water-cooling tungsten target module of rapid energy transfer fusion reactor divertor and cooling target plate structure |
| CN113897563A (en) * | 2021-10-08 | 2022-01-07 | 自贡硬质合金有限责任公司 | High-density tungsten alloy and preparation method thereof |
| CN114717491B (en) * | 2022-04-29 | 2022-12-02 | 中国科学院合肥物质科学研究院 | High-toughness W f /W composite material and preparation method thereof |
| CN114959518B (en) * | 2022-05-30 | 2023-01-31 | 合肥工业大学智能制造技术研究院 | Tungsten fiber and oxide nanoparticle synergistic toughening tungsten-based composite material and preparation method thereof |
| CN115404419B (en) * | 2022-09-20 | 2023-09-01 | 厦门钨业股份有限公司 | Preparation method of tungsten wire reinforced tungsten-based composite material |
| CN116460295B (en) * | 2023-04-27 | 2024-04-12 | 江苏科融新材料有限公司 | Preparation method of tungsten-lanthanum alloy wire |
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Address after: 230001 no.181 Gucheng Road, shiyangang Township, Hefei City, Anhui Province Patentee after: INSTITUTE OF PLASMA PHYSICS, CHINESE ACADEMY OF SCIENCES Address before: 230031 Shushan Lake Road, Shushan District, Anhui, China, No. 350, No. Patentee before: INSTITUTE OF PLASMA PHYSICS, CHINESE ACADEMY OF SCIENCES |